関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | (1,1'-Biphenyl)-2-ol | HCID 7017 | — |
| 反応物 | Phosphorus trichloride | HCID 24387 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 生成物 | 6H-Dibenz[c,e][1,2]oxaphosphorin, 6-chloro- | HCID 89816 | — |
反応手順
700 g (4.12 mol) of o-phenylphenol and 4.1 g of zinc chloride are heated to 180° C. with stirring. 692 g (5.03 mol) of phosphorus trichloride are then added dropwise over 12 hours. Reflux is maintained for a further 5 hours; at the end no further hydrogen chloride is evolved. The excess phosphorus trichloride is distilled off at 120° C. in vacuo, the reaction product is cooled to 100° C. and 966 g of toluene are added. Cooling to room temperature gives a 50% strength solution of 6-chloro-(6H)-dibenz[c,e][1,2]oxaphosphorin in toluene. The 31P-NMR spectrum indicates a purity of 95.5%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05391798 |
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| 出典データセット | uspto-grants-1995_02 |
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| ORD ID | ord-2f7c158a840b4861ba752948915936b2 |
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| 出典メモ | uspto-grants-1995_02 |
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